CN102923688B - Preparation method and application of nitrogen-doped carbon material - Google Patents
Preparation method and application of nitrogen-doped carbon material Download PDFInfo
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- CN102923688B CN102923688B CN201210430564.XA CN201210430564A CN102923688B CN 102923688 B CN102923688 B CN 102923688B CN 201210430564 A CN201210430564 A CN 201210430564A CN 102923688 B CN102923688 B CN 102923688B
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention provides a preparation method of a nitrogen-doped carbon material, which comprises the following steps: mixing Lewis acid and nitrogenous conductive polymer monomer, and reacting to obtain the nitrogen-doped carbon material. The nitrogenous conductive polymer monomer generates nitrogenous conductive polymer under the action of the Lewis acid, and the nitrogenous conductive polymer is activated to form pores under the action of the Lewis acid, thereby obtaining the nitrogen-doped carbon material. In the nitrogen-doped carbon material preparation process, the Lewis acid has the catalytic action on the polymerization of the nitrogenous conductive polymer monomer, and the acidic capacity of the Lewis acid promotes the activation and pore formation; and therefore, the nitrogen-doped carbon material can be prepared only by reacting the nitrogenous conductive polymer monomer and the Lewis acid, thereby simplifying the carbonization and activation process of the raw materials. The preparation method is simple.
Description
Technical field
The present invention relates to carbon material technical field, particularly relate to a kind of preparation method and application thereof of nitrogen-doped carbon material.
Background technology
Active carbon material be a kind of have enrich pore texture and the carbon material compared with bigger serface, it has the characteristic that chemical stability is good, mechanical property is high and conveniently can produce regeneration, has been widely used in gas delivery, purifying water process, catalytic chromatography analysis, energy storage and unmanageable engineering ceramics and the field such as has prepared.The active carbon material of functionalization, except having the character of active carbon, also has the purposes that other is more single-minded and special.Element doping is one of common functionalization mode, and the element for carbon material doping mainly contains the elements such as nitrogen, oxygen, boron, phosphorus.For nitrogen element, the carbon material after doping has particularly excellent performance in electrochemical catalysis field and energy storage field.
At present, the carbon material of nitrogen-doping mainly contains following several synthesis mode: doped in situ method, later stage activation method and carbonization-activation method.Doped in situ method is the carbon material adopting the organic molecule of Nitrogen element to carry out vapor deposition growth acquisition nitrogen-doping, this preparation method needs expensive plant and instrument, and the sample size of preparation is less, only can meet the needs of scientific research, cannot meet large-scale industrial production.Later stage activation rule is that the carbon material prepared is carried out later stage functionalization in the activated gas containing nitrogen element, but this reactivation process needs to complete at a higher temperature usually, therefore production energy consumption and safety factors are two large major issues of its development of restriction.Carbonization-activation method be by the organic polymer containing nitrogen element or biomass carbonated after carry out activation again.Prepare in the method for the carbon material of nitrogen-doping at above-mentioned three kinds, the concern that carbonization-activation method receives investigator because preparation condition is gentle, but the method often compares to be needed to carry out polystep reaction, preparation process more complicated, thus limits its widespread use.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of preparation method the preparation method of simple nitrogen-doped carbon material.
In view of this, the invention provides a kind of preparation method of nitrogen-doped carbon material, comprising:
Lewis acid is mixed with nitrogenous conductive polymers monomer, after reaction, obtains nitrogen-doped carbon material.
Preferably, described nitrogenous conductive polymers monomer and described lewis acidic mass ratio are 1:(0.1 ~ 10).
Preferably, described nitrogenous conductive polymers monomer is O-Phenylene Diamine, mphenylenediamine, Ursol D, aniline or pyrroles.
Preferably, described Lewis acid is iron(ic) chloride or Manganous chloride tetrahydrate.
Preferably, described reaction is carried out under protective atmosphere.
Preferably, the temperature of described reaction is 300 ~ 1000 DEG C, and the time of described reaction is 1 ~ 24h.
Preferably, also comprise after obtaining nitrogen-doped carbon material:
Described nitrogen-doped carbon material is washed in an acidic solution to pH be 6 ~ 7, dry.
Preferably, described acidic solution is hydrochloric acid or nitric acid.
Present invention also offers nitrogen-doped carbon material prepared by a kind of aforesaid method and prepare the application of electrode material for super capacitor.
Present invention also offers nitrogen-doped carbon material prepared by a kind of aforesaid method and prepare the application of lithium ion battery negative material.
The invention provides a kind of preparation method of nitrogen-doped carbon material, comprising: Lewis acid is mixed with nitrogenous conductive polymers monomer, after reaction, obtains nitrogen-doped carbon material.Nitrogenous conductive polymers monomer of the present invention generates nitrogenous conductive polymers under lewis acidic effect, and described nitrogenous conductive polymers carries out activation pore-creating under described lewis acidic effect subsequently, thus obtains nitrogen-doped carbon material.In the process preparing nitrogen-doped carbon material, because Lewis acid is to the katalysis of nitrogenous conductive polymers monomer polymerization, its acid ability facilitates activation pore-creating simultaneously, therefore the present invention only needs nitrogenous conductive polymers monomer and Lewis acid to react can prepare nitrogen-doped carbon material, simplify the process of raw material charing and activation, thus make the preparation method of nitrogen-doped carbon material simple.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram of nitrogen-doped porous carbon material prepared by the embodiment of the present invention 1;
Fig. 2 is that the ultimate analysis XPS of nitrogen-doped porous carbon material prepared by the embodiment of the present invention 1 schemes;
Fig. 3 is the nitrogen adsorption desorption graphic representation of nitrogen-doped porous carbon material prepared by the embodiment of the present invention 1;
Fig. 4 is the constant current charge-discharge graphic representation of nitrogen-doped porous carbon material under the current density of 0.1A/g prepared by the embodiment of the present invention 1;
Fig. 5 is nitrogen-doped porous carbon material 0.1mA/cm prepared by the embodiment of the present invention 1
2current density under storage lithium performance chart.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The embodiment of the invention discloses a kind of preparation method of nitrogen-doped carbon material, comprising:
Lewis acid is mixed with nitrogenous conductive polymers monomer, after reaction, obtains nitrogen-doped carbon material.
According to the present invention, described nitrogenous conductive polymers monomer is preferably aniline, O-Phenylene Diamine, Ursol D, mphenylenediamine or pyridine, and described nitrogenous conductive polymers monomer, under lewis acidic katalysis, obtains nitrogenous conductive polymers.In described conductive polymers, long-range continuous print conjugated structure imparts the electron transport ability of conductive polymers excellence; In nitrogenous conductive polymers, abundant heteroatoms is also conducive to the lifting of electroconductibility simultaneously, therefore, present invention employs nitrogenous conductive polymers monomer as the raw material preparing nitrogen-doped carbon material.Described Lewis acid has acidity and the effect of activation pore-creating, and mixed with Lewis acid by nitrogenous conductive elements polymkeric substance, described Lewis acid has katalysis to described nitrogenous conductive polymers monomer polymerization, thus obtains nitrogenous conductive polymers; Subsequently due to lewis acidic activation pore-creating effect, described nitrogenous conductive polymers is carried out active pore-creating, thus obtain the nitrogen-doped carbon material of porous.Described Lewis acid is preferably iron(ic) chloride, Manganous chloride tetrahydrate, Potcrate or Potassium Iodate.
Because described lewis acidic consumption has larger impact to the pore diameter characteristics of prepared nitrogen-doped carbon material and the conservation rate of nitrogen element, described nitrogenous conductive polymers monomer and described lewis acidic mass ratio are preferably 1:(0.1 ~ 10), be more preferably 1:(0.5 ~ 8), most preferably be 1:(2 ~ 5).Preferably, after described nitrogenous conductive polymers monomer mixes with described Lewis acid, proceed in High Temperature Furnaces Heating Apparatus by it and react.In order to prevent the oxygen reaction in the element such as nitrogen, carbon and air, generate carbonic acid gas, carbon monoxide or nitrogen oxide, described reaction is preferably carried out under protective atmosphere, is more preferably and carries out under nitrogen or argon gas atmosphere.The temperature of described reaction is preferably 300 ~ 1000 DEG C, is more preferably 500 ~ 800 DEG C, if temperature of reaction is too low, is unfavorable for the catalyzed polymerization of described Lewis acid to described nitrogenous conductive polymers monomer, if described temperature is too high, is then unfavorable for the stable doping of nitrogen element.The time of described reaction is preferably 1 ~ 24h, is more preferably 2 ~ 10h.
According to the present invention, preferably, after prepared by described nitrogen-doped carbon material, then described nitrogen-doped carbon material is washed in an acidic solution to pH be 6 ~ 7, to remove the impurity such as unnecessary metal ion.Described acidic solution is preferably hydrochloric acid or nitric acid.
Nitrogenous conductive polymers monomer of the present invention generates nitrogenous conductive polymers under lewis acidic effect, and described conductive polymers carries out activation pore-creating under the effect of described Lewis acid acidity subsequently, thus obtains the nitrogen-doped carbon material of porous.In the process preparing nitrogen-doped carbon material, because Lewis acid is to the katalysis of nitrogenous conductive polymers monomer polymerization, simultaneously its acid ability is that the activation pore-creating of nitrogenous conductive polymers provides conveniently, therefore the present invention only needs nitrogenous conductive polymers monomer and Lewis acid to react can prepare nitrogen-doped carbon material, simplify the process of raw material charing and activation, preparation method is simple.Experiment shows, the nitrogen-doped carbon material prepared by the present invention has abundant pore structure, larger specific surface area and abundant nitrogen-doping.
Present invention also offers described nitrogen-doped carbon material and prepare the application of electrode material for super capacitor.Preparation method the present invention of described electrode of super capacitor has no particular limits, and is preparation method well known to those skilled in the art, the nitrogen-doped carbon material that what just electrode materials was selected is prepared by the present invention.The electrochemical capacitor performance of the present invention by adopting cyclic voltammetry to test described nitrogen-doped carbon material electrodes, experimental result shows, described nitrogen-doped carbon material has typical electric double layer capacitance and fake capacitance behavior, under potential region is-0.7 ~ 0 volt with the electrochemistry capacitance under the current density constant current charge-discharge of 0.1A/g for 690F/g.
Present invention also offers and the nitrogen-doped carbon material of preparation is being prepared the application of negative material of lithium ion battery.Equally, the preparation method of the present invention to described lithium ion battery negative has no particular limits, and is mode well known to those skilled in the art, and just negative material is nitrogen-doped carbon material prepared by the present invention.The present invention adopts constant current charge-discharge method to investigate the storage lithium performance of nitrogen-doped carbon material, and result shows, described nitrogen-doped carbon material has excellent storage lithium characteristic, with 0.1mA/cm in 0 ~ 3 volt of interval
2speed continuous current circulation time, its capacity can reach 900mAhg
-1.
In order to understand the present invention further, be described in detail to nitrogen-doped carbon material provided by the invention and application thereof below in conjunction with embodiment, protection scope of the present invention is not limited by the following examples.
Embodiment 1
After commercial O-Phenylene Diamine is mixed with mass ratio 1:5 with commercial iron trichloride, proceed in High Temperature Furnaces Heating Apparatus, under argon atmospher protection; 6 hours are processed under 500 degrees Celsius; cool the hydrochloric acid soln washing of rear 2M to remove metal ion, dry, obtain the nitrogen-doped carbon material of porous.
Utilize scanning electronic microscope, elemental analyser, the analysis of gas adsorption desorption carries out physico-chemical property test to prepared nitrogen-doped carbon material, as shown in Figure 1, Figure 2 and Figure 3, Fig. 1 is the electron scanning micrograph of nitrogen-doped porous carbon material to characterization result; Fig. 2 is that the ultimate analysis XPS of nitrogen-doped porous carbon material schemes; Fig. 3 is the nitrogen adsorption desorption graphic representation that the embodiment of the present invention 1 prepares nitrogen-doped porous carbon material; Carry out electrochemical capacitor test and the performance test of storage lithium to the nitrogen-doped porous carbon material of preparation, as shown in Figure 4 and Figure 5, Fig. 4 is the constant current charge-discharge figure of nitrogen-doped porous carbon material under the current density of 0.1A/g to test result; Fig. 5 is nitrogen-doped porous carbon material 0.1mA/cm
2current density under storage lithium performance chart.
From Fig. 1, Fig. 2 and Fig. 3, described nitrogen-doped porous carbon material specific surface area is 591m
2g
-1, pore size is mainly the micropore being less than 2nm, and part is mesoporous is greater than 2nm; Ultimate analysis atomic percent is carbon element content is 83%, and oxygen element content is 8.6%, and nitrogen element content is 8.4%.From Fig. 4 and Fig. 5, nitrogen-doped carbon material is at 1M H
2sO
4-electrochemistry capacitance in ionogen is 690Fg
-1, the storage lithium performance of nitrogen-doped carbon material is 650mAhg
-1.
Embodiment 2
After O-Phenylene Diamine is mixed with mass ratio 1:5 with iron trichloride, proceed in High Temperature Furnaces Heating Apparatus, under argon atmospher protection, under 700 degrees Celsius, process 6 hours, cool the hydrochloric acid soln washing of rear 2M to remove metal ion, drying and gained.
Experimental result shows: nitrogen-doped porous carbon material specific surface area is 320m
2g
-1, pore size is based on mesoporous; Ultimate analysis atomic percent is carbon element content is 94.4%, and oxygen element content is 1.2%, and nitrogen element content is 4.4%.Nitrogen-doped carbon materials application in the test result of ultracapacitor be 498Fg
-1.The storage lithium performance of nitrogen-doped carbon material is 780mAhg
-1.
Embodiment 3
After Ursol D is mixed with mass ratio 1:6 with iron trichloride, proceed in High Temperature Furnaces Heating Apparatus, under argon atmospher protection, under 500 degrees Celsius, process 10 hours, cool the hydrochloric acid soln washing of rear 2M to remove metal ion, drying and gained.
Experimental result shows: nitrogen-doped porous carbon material specific surface area is 985m
2g
-1, pore size is mainly the micropore being less than 2nm; Ultimate analysis atomic percent is carbon element content is 85.2%, and oxygen element content is 7.2%, and nitrogen element content is 7.6%.The test result that nitrogen-doped carbon material is used for ultracapacitor is 450Fg
-1.The storage lithium performance of nitrogen-doped carbon material is 900mAhg
-1.
Embodiment 4
After mphenylenediamine is mixed with mass ratio 1:2 with iron trichloride, proceed in High Temperature Furnaces Heating Apparatus, under argon atmospher protection, under 450 degrees Celsius, process 8 hours, cool the hydrochloric acid soln washing of rear 2M to remove metal ion, drying and gained.
Experimental result shows: nitrogen-doped porous carbon material specific surface area is 200m
2g
-1, pore size is mainly the micropore being less than 2nm; Ultimate analysis atomic percent is result carbon element content is 84.5%, and oxygen element content is 6.8%, and nitrogen element content is 8.7%.It is 298Fg that nitrogen-doped carbon material is used for ultracapacitor test result
-1.The storage lithium performance of nitrogen-doped carbon material is 470mAhg
-1.
Embodiment 5
After pyrroles is mixed with mass ratio 1:8 with iron trichloride, proceed in High Temperature Furnaces Heating Apparatus, under argon atmospher protection, under 350 degrees Celsius, process 10 hours, cool the hydrochloric acid soln washing of rear 2M to remove metal ion, drying and gained.
Experimental result shows: nitrogen-doped porous carbon material specific surface area is 185m
2g
-1, pore size is mainly the micropore being less than 2nm; Ultimate analysis atomic percent is the content of carbon is 83.8%, and the content of oxygen element is 7.4%, and the content of nitrogen element is 8.8%.It is 560Fg that nitrogen-doped carbon material is used for ultracapacitor test result
-1.The storage lithium performance of nitrogen-doped carbon material is 670mAhg
-1.
The explanation of above embodiment just understands method of the present invention and core concept thereof for helping.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improve and modify and also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (4)
1. a preparation method for nitrogen-doped carbon material, is characterized in that, comprising:
Lewis acid is mixed with nitrogenous conductive polymers monomer, after reaction, obtains nitrogen-doped carbon material;
Described nitrogenous conductive polymers monomer is O-Phenylene Diamine, mphenylenediamine, Ursol D, aniline or pyrroles; Described Lewis acid is iron(ic) chloride, Manganous chloride tetrahydrate, Potcrate or Potassium Iodate;
Described nitrogenous conductive polymers monomer and described lewis acidic mass ratio are 1:(0.1 ~ 10);
Described reaction is carried out under protective atmosphere.
2. preparation method according to claim 1, is characterized in that, the temperature of described reaction is 300 ~ 1000 DEG C, and the time of described reaction is 1 ~ 24h.
3. preparation method according to claim 1, is characterized in that, also comprises after obtaining nitrogen-doped carbon material:
Described nitrogen-doped carbon material is washed in an acidic solution to pH be 6 ~ 7, dry.
4. preparation method according to claim 3, is characterized in that, described acidic solution is hydrochloric acid or nitric acid.
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| CN103072972B (en) * | 2013-03-04 | 2014-06-11 | 兰州理工大学 | Preparation method of nitrogen and sulfur co-doping ordered mesoporous carbon materials |
| CN103072973B (en) * | 2013-03-04 | 2014-06-11 | 兰州理工大学 | Preparation method of nitrogen-doping ordered mesoporous carbon materials |
| CN103130206B (en) * | 2013-03-05 | 2015-03-04 | 东北林业大学 | Nitrogen doped carbon material and preparation method |
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| CN107308975A (en) * | 2017-07-07 | 2017-11-03 | 江南大学 | A kind of preparation method of nitrogen-doped carbon package metals oxide catalyst |
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| CN111790350B (en) * | 2020-05-26 | 2022-04-26 | 福州大学 | Preparation method of nitrogen-doped carbon material and application of nitrogen-doped carbon material in removal of sulfur-containing gas |
| CN111960403B (en) * | 2020-08-31 | 2023-02-17 | 西南大学 | Preparation method of coal tar-based nitrogen-doped porous carbon material, product thereof and application of product in super capacitor |
| CN112952096B (en) * | 2021-02-18 | 2022-09-02 | 广东佳纳能源科技有限公司 | Nitrogen-doped carbon-coated lithium ion battery positive electrode material and preparation method thereof |
| CN115672267B (en) * | 2021-07-27 | 2024-05-17 | 无锡蓝海工程设计有限公司 | Nitrogen-doped carbon material, preparation method thereof and application thereof in heavy metal ion adsorption |
| CN115432702B (en) * | 2022-08-18 | 2023-06-23 | 同济大学 | Method for preparing carbon super-structure material based on Lewis acid-base interaction self-assembly |
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